CN102507570A - Method for determining chemical oxygen demand (COD) of titanium dioxide production waste water - Google Patents
Method for determining chemical oxygen demand (COD) of titanium dioxide production waste water Download PDFInfo
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- CN102507570A CN102507570A CN2011103339729A CN201110333972A CN102507570A CN 102507570 A CN102507570 A CN 102507570A CN 2011103339729 A CN2011103339729 A CN 2011103339729A CN 201110333972 A CN201110333972 A CN 201110333972A CN 102507570 A CN102507570 A CN 102507570A
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- chemical oxygen
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Abstract
The invention relates to a method for determining chemical oxygen demand (COD) of titanium dioxide production waste water, which belongs to the field of titanium dioxide production and comprises the steps of A neutralizing titanium dioxide waste water through alkali; B determining the chemical oxygen demand of neutralized titanium dioxide waste water through a potassium dichromate method, wherein the reaction time for heating return flow is 10-30 minutes; C enabling the titanium dioxide waste water with unqualified chemical oxygen demand to repeat the step of A. By means of the method for determining a value of the COD, under the premise of an accurate test value, the operation is simple and easy to implement and the analysis process is fast and effective. Therefore, the method can be widely applied to the detection of the COD of the titanium dioxide waste water.
Description
Technical field
The invention belongs to the titanium white production field, be specifically related to a kind of assay method of Producing Titanium Dioxide chemical oxygen demand of waste water.
Background technology
COD (Chemical Oxygen Demand) is a COD, and COD is chemically to measure the amount that needs oxidized reducing substances in the water sample.It has reflected the degree that polluted by reducing substances, and the COD value is high more, and organic pollutants are heavy more in the expression water; Reducing substances mainly is various organism in the water, also has a spot of nitrite, sulfide, ferrous salt etc.
Existing potassium dichromate method is measured COD and is common to all waste water COD checks, is specially: in acid medium, be oxygenant with the potassium dichromate; Silver sulfate is a catalyzer; Mercuric sulfate is the screening agent of chlorion, behind water cooling backflow reacting by heating 2h, is indicator with the ferroin; With the remaining potassium dichromate of l ferrous ammonium sulfate solution titration, according to the COD value of the consumption calculating water sample of l ferrous ammonium sulfate solution; Referring to GB11914-89.
It is thus clear that, need reflux 2h when existing potassium dichromate method is measured in the water sample COD value, consuming time longer, in the Producing Titanium Dioxide process, the wastewater treatment personnel can not know in time that whether qualified the COD index is, and the guidance of water quality regulation is seriously lagged behind.
Summary of the invention
The technical matters that the present invention will solve provides a kind of assay method of COD (COD) of Producing Titanium Dioxide waste water, and solve titanium dioxide wastewater COD and detected problem slowly, and the numerical value basically identical of COD numerical value that draws and prior art mensuration.
Technical scheme of the present invention is:
The invention provides a kind of assay method of COD (COD) of Producing Titanium Dioxide waste water, concrete steps are:
A uses the alkali neutralisation treatment with titanium dioxide wastewater;
Titanium dioxide wastewater after the B neutralisation treatment is measured COD with potassium dichromate method, and this method comprises the backflow heating steps, and wherein, the backflow reacting by heating time is 10-30min;
The titanium dioxide wastewater of C COD>100mg/l is back to the A step.
Preferably, in the assay method of the COD of above-mentioned Producing Titanium Dioxide waste water (COD), the backflow reacting by heating time is 10min.
Beneficial effect of the present invention:
Utilize the inventive method to measure the COD value of Producing Titanium Dioxide waste water, accurately under the prerequisite, easy to operation, the analytic process effective and rapid can be widely used in the titanium dioxide wastewater COD detection at test value.
Embodiment
The invention provides a kind of assay method of COD (COD) of Producing Titanium Dioxide waste water, be specially:
A uses the alkali neutralisation treatment with titanium dioxide wastewater;
Titanium dioxide wastewater after the B neutralisation treatment is measured COD with potassium dichromate method, and this method comprises the backflow heating steps, and wherein, the backflow reacting by heating time is 10-30min;
The titanium dioxide wastewater of C COD>100mg/l is back to the A step.
Potassium dichromate method is measured COD and is specially:
Efflux wastewater appearance after the neutralisation treatment is stirred, get 10ml, place the backflow conical flask of 250ml ground; Accurately add 10ml potassium dichromate standard solution and 100 above beaded glasses; Slowly add 20ml sulfuric acid-silver sulfate, electric furnace voltage is transferred to 200V, after the boiling; Turn electric furnace voltage down and keep little boiling, backflow 10min at 100-150V.Close electric furnace, the cooling 3min that continues to reflux with suitable quantity of water flushing condensation tube wall, takes off conical flask, and adding distil water is diluted to about 140ml.Add 3 ferroin indicator, use the iron ammonium sulfate titration, solution colour is extremely tenne through blue-green by yellow to be terminal point.
Simultaneously, do blank by same operation steps with the 10ml redistilled water.
The result calculates
COD=C×(V
0-V
1)×8×1000/V
The N of C-iron ammonium sulfate standard solution, mol/L
V
0Consume the volume of iron ammonium sulfate standard solution during-blank titration, ml
V
1Consume the volume of iron ammonium sulfate standard solution during the titration of-waste water appearance, ml
V-waste water appearance volume, ml
Can get COD numerical value by following formula calculating, if numerical value≤100mg/l, then COD is qualified; Defective otherwise (referring to standard GB 18918-2002).
Measure in the prior art that COD all adopts the potassium dichromate method of stipulating among the GB11914-89 in the waste water, and also clearly indicated in the method the need reflux in this regulation 2 hours.Since national standard so stipulates, people in measuring waste water during COD naturally all according to this standard implementation, and do not have motivation to go to adopt to shorten the reflux time or other means go to change COD method of testing of the prior art.The present invention is directed to the titanium white field; Overcome technological prejudice; When titanium dioxide wastewater being adopted potassium dichromate method measure in the water sample COD value, only need reflux 10-30min after the alkali neutralisation treatment, and can guarantee that test result is correct, show method of testing effective and rapid of the present invention; And, utilize this method to measure COD value of waste water, the wastewater treatment personnel can know in time that whether qualified the COD index is, so that in time instruct the adjusting to water quality.
Do further description below in conjunction with the embodiment specific embodiments of the invention, therefore do not limit the present invention among the described scope of embodiments.
Material and instrument
Potassium dichromate standard solution C (1/6K
2Cr
2O
7)=0.25mol/L is with 12.2580g K
2Cr
2O
7Be dissolved in water the back constant volume in the 1000ml volumetric flask.
Ferroin indicator 1.485g Phen (C
12H
8.H
2O) with 0.695g ferrous sulphate (FeSO
4.7H
2O) water-soluble, be diluted to 100ML and shake up, store in the brown bottle.
Iron ammonium sulfate standard solution 0.1mol/L is soluble in water the 39.2g iron ammonium sulfate, adds the 30ml concentrated sulphuric acid, and constant volume is in the 1000ml volumetric flask.
Sulfuric acid-silver sulfate: the 5g silver sulfate is joined in the 500ml concentrated sulphuric acid, stir and make it dissolving.
Reflux 500ml spherical condensation tube
Electric furnace 220V 1KW
Embodiment 1
The waste water of being selected for use is: one batch of efflux wastewater after the neutralisation treatment of Panzhihua ancient cooking vessel star titanium industry company.
With waste water in lime and after, stir, get 10ml; Place the backflow conical flask of 250ml ground, accurately add 10ml potassium dichromate standard solution and 100 above beaded glasses, slowly add 20ml sulfuric acid-silver sulfate; Electric furnace voltage is transferred to 200V; After the boiling, turn electric furnace voltage down and keep little boiling at 100-150V, return time is respectively 5min, 10min, 15min, 30min, 2h.Close electric furnace, continue backflow 3min, with suitable quantity of water flushing condensation tube wall, take off conical flask, adding distil water is diluted to about 140ml.Add 3 ferroin indicator, use the iron ammonium sulfate titration, solution colour is extremely tenne through blue-green by yellow to be terminal point.Simultaneously, do blank by same operation steps with the 10ml redistilled water.The result is as shown in table 1.
Embodiment 2
Choose two batches of (with one batch of asynchronism(-nization)) efflux wastewaters after the neutralisation treatment of Panzhihua ancient cooking vessel star titanium industry company, other steps are with embodiment 1.
Embodiment 3
Choose three batches of efflux wastewaters after the neutralisation treatment of Panzhihua ancient cooking vessel star titanium industry company, other steps are with embodiment 1.
Comparative Examples
In addition, we adopt the existing reflux time is 2h, and other steps have been measured its COD value with embodiment 1 to three batches of efflux wastewaters, and its result is as shown in table 2.
In addition, the present invention has also adopted oxydol titration ocular estimate to measure the COD of titanium dioxide wastewater, promptly gets efflux wastewater 20ml, adds several oxydol, and observation waste water change color is constant until color, generally needs 10s; If be colourless finally, then COD is qualified basically; If faint yellow, show that COD numerical value is lower; If yellow, show that COD is defective; The result is as shown in table 3.
COD value under the table 1 different heating return time
The 5minCOD value | The 10minCOD value | The 15minCOD value | The 30minCOD value | |
Embodiment 1 | 38.1 | 51.26 | 51.4 | 51.0 |
Embodiment 2 | 45.7 | 55.78 | 55.5 | 55.4 |
Embodiment 3 | 50.2 | 60.42 | 60.1 | 60.2 |
Table 2 contrast test
The 2hCOD value | |
Comparative Examples 1 | 51.15 |
Comparative Examples 2 | 55.01 |
Comparative Examples 3 | 60.41 |
The COD value of table 3 oxydol titration range estimation titanium dioxide wastewater
Change color behind the adding oxydol | COD judges | |
One batch of waste water | Colourless | Qualified |
Two batches of waste water | Colourless | Qualified |
Three batches of waste water | Colourless | Qualified |
Can know by table 1-table 3, utilize the COD value of waste water that titanium dioxide wastewater COD value that assay method of the present invention records and prior art potassium dichromate method record and the basically identical as a result of ocular estimate, and method required time of the present invention significantly reduce.
Claims (2)
1. the assay method of the COD of Producing Titanium Dioxide waste water, concrete steps are:
A uses the alkali neutralisation treatment with titanium dioxide wastewater;
Titanium dioxide wastewater after the B neutralisation treatment is measured COD with potassium dichromate method, and this method comprises the backflow heating steps, and wherein, the backflow reacting by heating time is 10-30min;
The titanium dioxide wastewater of C COD>100mg/l is back to the A step.
2. the assay method of the COD of Producing Titanium Dioxide waste water according to claim 1 is characterized in that: the said backflow reacting by heating time is 10min.
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Cited By (3)
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CN104280384A (en) * | 2014-06-24 | 2015-01-14 | 浙江富春环保新材料有限公司 | Method for accurately measuring COD value of wastewater generated through strip steel hydrochloric acid pickling process |
CN107589086A (en) * | 2017-08-29 | 2018-01-16 | 南京工业大学 | A kind of hydrogen peroxide remover composition, removing method and quick COD assay methods for COD measure |
CN109521143A (en) * | 2018-11-23 | 2019-03-26 | 绍兴市中测检测技术股份有限公司 | Organic wastewater COD online test method |
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CN1598548A (en) * | 2004-08-05 | 2005-03-23 | 大连交通大学 | Quick detecting method for needed oxygen COD cr of mercuryless salt high-chlorine waste water chemical |
CN101750414A (en) * | 2008-12-09 | 2010-06-23 | 周建飞 | Method for measuring chemical oxygen demand of waste water |
CN101858869A (en) * | 2010-05-14 | 2010-10-13 | 杭州华集环境检测技术有限公司 | Air flow-back detection method for chemical oxygen demand (COD) in water |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104280384A (en) * | 2014-06-24 | 2015-01-14 | 浙江富春环保新材料有限公司 | Method for accurately measuring COD value of wastewater generated through strip steel hydrochloric acid pickling process |
CN107589086A (en) * | 2017-08-29 | 2018-01-16 | 南京工业大学 | A kind of hydrogen peroxide remover composition, removing method and quick COD assay methods for COD measure |
CN107589086B (en) * | 2017-08-29 | 2019-08-23 | 南京工业大学 | A kind of hydrogen peroxide remover composition, removing method and quick COD measuring method for COD measurement |
CN109521143A (en) * | 2018-11-23 | 2019-03-26 | 绍兴市中测检测技术股份有限公司 | Organic wastewater COD online test method |
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Application publication date: 20120620 |